A crude oil direct oiling type spinning oil, a preparation method and application thereof

Abstract

The application provides a crude oil direct oiling type spinning oil, a preparation method and application. The crude oil direct oiling type spinning oil comprises 65-75% of a composite smoothing agent, and the composite smoothing agent is composed of tetradecyl tetradec-9-enoate 25-35 parts and PEG-12 dipalmitate 65-75 parts. The composite smoothing agent is composed of specific compounds, so that the spinning oil can have smoothness, oil film strength and heat resistance; meanwhile, the friction coefficient of the yarn can be reduced and the uniformity of the yarn can be improved, and the quality of the yarn is good.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of spinning, in particular to a crude oil direct oiling type spinning oil agent, a preparation method and application. BACKGROUND

[0002] As the synthetic fiber product category with the largest global production capacity and the most widely application, the mainstream preparation method of polyester is to integrate high-speed spinning (spinning speed up to 2600-3500 m / min) with ultra-high-speed drawing and winding (winding speed up to 5100-5500 m / min) into a one-step spinning and drawing method, which not only significantly reduces production cost, but also performs outstandingly in product quality stability, providing strong support for efficient and high-quality development of the polyester industry.

[0003] In the entire processing process, the spinning oil agent not only needs to ensure that each manufacturing and processing procedure can smoothly and unobstructedly proceed, but also needs to ensure that the fiber quality is not affected at all. Since the traditional spinning process usually adopts an emulsion oiling type oil agent, taking mineral oil as base oil, the spinning oil agent crude oil needs to be first mixed with water to form an emulsion before use. In the actual spinning process, in order to promote the evaporation of water in the oil agent, the temperature of the fiber passing through the hot roller needs to be increased, which consumes a large amount of energy and causes serious waste of energy; and with the evaporation of water, the oil film is easily damaged, thereby causing the rupture of the oil film on the fiber surface and ultimately causing uneven oiling, which seriously affects the fiber quality.

[0004] Therefore, the Chinese patent with application number 202311223821.7 discloses a crude oil oiling type FDY spinning oil agent, which comprises 40wt%-60wt% of a smoothing agent, 15wt%-40wt% of an emulsifier, 1wt%-5wt% of an antistatic agent, 1wt%-10wt% of a wetting penetrant and 5wt%-10wt% of water, wherein the average molecular weight of the wetting penetrant is less than or equal to 2000, the HLB value of the wetting penetrant is less than or equal to 6, and the HLB value of the emulsifier is 3-15. The crude oil oiling type FDY spinning oil agent in the present application reduces the surface tension of the crude oil oiling type FDY spinning oil agent under the synergistic action of the wetting penetrant and the emulsifier, so that the crude oil oiling type FDY spinning oil agent has excellent wetting spreading property and permeability. However, the above spinning oil agent is difficult to maintain the required thermal stability in the high-speed spinning process, resulting in poor uniformity and smoothness of the yarn and prone to yarn breakage.

[0005] Therefore, the present application is proposed. SUMMARY

[0006] The problem solved by the present application is that the existing crude oil direct oiling type spinning oil agent is difficult to maintain the required thermal stability and emulsion stability, resulting in poor quality of the produced yarn.

[0007] To solve the above problems, the present application provides a crude oil direct oiling type spinning oil, comprising 65-75% of a composite smoothing agent, the composite smoothing agent consisting of tetradecyl tetradec-9-enoate 25-35 parts, PEG-12 dipalmitate 65-75 parts.

[0008] Preferably, the crude oil direct oiling type spinning oil consists of the composite smoothing agent 65-75 parts, emulsifier 10-15 parts, penetrant 2-4 parts, antistatic agent 2-6 parts, solvent 6-10 parts, wherein the composite smoothing agent consists of tetradecyl tetradec-9-enoate 25-35 parts, PEG-12 dipalmitate 65-75 parts, and the solvent is water.

[0009] Preferably, the emulsifier is at least one selected from fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, cardanol polyoxyethylene ether, castor oil polyoxyethylene ether, sorbitan fatty acid ester, sorbitan polyoxyethylene ether fatty acid ester or polyethylene glycol fatty acid ester.

[0010] Preferably, the penetrant is at least one selected from fatty alcohol polyoxyethylene ether, potassium perfluorooctylsulfonate, sodium perfluorooctylsulfonate. Preferably, the penetrant consists of sodium perfluorooctylsulfonate and potassium perfluorooctylsulfonate in a mass ratio of 1:2.

[0011] Preferably, the antistatic agent is at least one selected from alkyl alcohol phosphate polyoxyethylene ether, alkyl alcohol phosphate, alkyl alcohol sulfonate, alkyl alcohol polyoxyethylene ether sulfonate, alkyl alcohol sulfate, alkyl alcohol ether sulfate and alkyl alcohol ether carboxylate fatty amine polyoxyethylene ether, alkyl alcohol ammonium oxide or betaine.

[0012] Preferably, the pH of the crude oil direct oiling type spinning oil is 7.5-8.0.

[0013] The present application also provides a preparation method of the crude oil direct oiling type spinning oil, comprising the following steps: adjusting the temperature in the reaction kettle to 38-45℃, adding the composite smoothing agent by quantity, stirring at 800-1400 rad / min for 10-50 min, then adding the antistatic agent and stirring for 10-40 min, then adding the solvent and the penetrant and stirring for 20-50 min, finally adding the emulsifier and stirring for 30-90 min, cooling to room temperature, and then filtering to obtain the crude oil direct oiling type spinning oil.

[0014] Preferably, the preparation method of the crude oil direct oiling type spinning finish comprises the following steps: adjusting the temperature in the reaction kettle to 40-45 DEG C, adding the composite smoothing agent in a certain amount, stirring at 800-1200 rad / min for 10-30 min, then adding the antistatic agent and stirring for 10 min, then adding the solvent and the penetrating agent and stirring for 20-40 min, finally adding the emulsifier and stirring for 30-60 min, filtering after cooling to room temperature, and the crude oil direct oiling type spinning finish is obtained.

[0015] The application further discloses application of the crude oil direct oiling type spinning finish in a spinning production process.

[0016] Compared with the prior art, the crude oil direct oiling type spinning finish, the preparation method and the application have the following beneficial effects: 1) the components of the composite smoothing agent are optimized from the aspects of the number of carbon atoms, the saturation degree and the number of hydroxyl groups, so that the spinning finish can have the smoothness, the oil film strength and the heat resistance; 2) the PEG-12 dipalmitate is used to replace the mineral oil, so that the friction coefficient of the yarn is reduced and the uniformity of the yarn is improved, and the quality of the yarn is good; 3) by selecting a specific feeding sequence, the spinning finish has good light transmittance and good emulsion stability; and 4) by selecting a specific penetrating agent, the surface tension of the final spinning finish can be significantly reduced, so that the oil dirt generated under the high-temperature condition is effectively prevented from being accumulated on the radiant heat heater, the yarn breakage rate is significantly reduced, the cleaning cycle of the heater is prolonged, and the production continuity is high. DETAILED DESCRIPTION

[0017] The application will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are used to illustrate the application but not to limit the scope of the application. Furthermore, it should be understood that those skilled in the art can make various modifications or changes to the application after reading the content of the application, and these equivalent forms also fall within the scope of the appended claims of the application.

[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the application herein is for the purpose of describing particular embodiments or examples only and is not intended to be limiting of the application. The materials, reagents and equipment involved in the embodiments of the application are commercially available unless otherwise specified.

[0019] The conventional FDY spinning process mainly uses an emulsion type spinning finish. Since the crude oil spinning finish needs to be mixed with water to form an emulsion before use, the water in the spinning finish is evaporated by increasing the temperature of the hot roller in the spinning process, and there are disadvantages such as high energy consumption, reduced heat conduction efficiency of the yarn, limitations of water dilution on the composition of the spinning emulsion, and changes in the physical properties of the yarn caused by water input and output.

[0020] For this direct oiling type spinning oil is developed, which not only requires the fiber adhesion comparable to the traditional emulsion, but also can maintain the required thermal stability and emulsion stability in the high-speed spinning process to ensure the quality of the final yarn stable controllable. The smoothing agent in the spinning oil is mainly used to reduce the friction resistance between the fiber and the spinning equipment, the emulsifier is mainly to balance the monomers in the oil agent through physical and chemical process to ensure that it can become a uniform and stable emulsion when used, the penetrating agent is the main component to reduce the surface tension of the oil agent, so that the oil agent is more easily evenly covered on the surface of the fiber, the antistatic agent is used to reduce the charge accumulation, prevent the fiber from generating static electricity in the spinning process, the above components jointly determine the high temperature stability, emulsion stability of the oil agent, and are also important factors to ensure the quality of the yarn stable. Therefore, the applicant proposes the following technical scheme:

[0021] Experimental example Optimization of composite smoothing agent

[0022] The smoothing agent is one of the core components of the spinning oil, which can not only reduce or control the friction generated during the contact and operation of the fiber on the surface of the textile equipment made of various materials including metal, but also has an impact on the smoothness, oil film strength, heat resistance and even viscosity of the final oil agent. The current smoothing agent is usually selected from a certain index, which cannot take into account multiple performance parameters of the oil agent. The applicant optimizes the composition A of the composite smoothing agent according to Table 1 and prepares the spinning oil according to the method of Example 1.

[0023] The oil film strength, thermal stability of the prepared spinning oil and the static friction coefficient of the prepared filament are measured by the following method, wherein the oil film strength is characterized by the maximum non-engaging force tested by a four-ball friction tester, the thermal stability is characterized by the residual percentage after 1.0 ml of the oil agent sample is dropped on a steel test piece and placed in an oven at 230°C for 40 minutes, and the static friction coefficient between the above filament and metal is measured under the condition of 300g load and 0.2rpm. The specific test method is the prior art, which is not described here.

[0024] Table 1 Influence of composite smoothing agent composition on oil agent performance

[0025]

[0026] Table 1 shows that when the number of carbon atoms in the linear alcohol in component A is high or low, the static friction coefficient of the final filament is high, indicating poor smoothness of the oil. When the number of hydroxyl groups in the linear alcohol in component A is 2, the evaporation loss is low, indicating poor thermal stability. Furthermore, for the fatty acids in component A, when the number of carbon atoms is low, the oil film strength is low, making yarn breakage more likely; while when the number of carbon atoms is high, the static friction coefficient of the final filament is high, indicating poor smoothness of the oil. When saturated fatty acids are used, the evaporation loss is low, indicating poor thermal stability. In summary, the oil prepared using tetradecyltetradec-9-enoate as one of the components of the composite smoother in this application can balance oil film strength and thermal stability while exhibiting good smoothness.

[0027] Example 1

[0028] A crude oil-based spinning oiling agent comprises the following components: 75 parts of a composite smoothing agent, 10 parts of an emulsifier, 4 parts of a penetrant, 2 parts of an antistatic agent, and 9 parts of a solvent. The composite smoothing agent comprises 35 parts of tetradecyl tetradecyl-9-enoate and 65 parts of PEG-12 dispalmitate. The emulsifier is PEG-400 monooleate. The penetrant is fatty alcohol polyoxyethylene ether. The antistatic agent is alkyl alcohol phosphate polyoxyethylene ether. The solvent is water.

[0029] The following method was used to prepare the product: After adjusting the temperature inside the reactor to 40°C, tetradecyl tetradec-9-enoate and PEG-12 dispalmitate were added and stirred at 1000 rad / min for 10 min. Then, alkyl alcohol phosphate polyoxyethylene ether was added and stirred for 10 min. After that, water and fatty alcohol polyoxyethylene ether were added and stirred for 20 min. Finally, emulsifier PEG-400 monooleate was added and stirred for 30 min. After cooling to room temperature, the product was filtered to obtain the final product.

[0030] The tetradecyl tetradec-9-enoate (myristyl myristoleate) is prepared by the following method: Myristyl alcohol (C 14 H 29 OH) and myristoleic acid (tetradecanoic acid, C 14 H 26 O2) is added to the reactor at a molar ratio of 1:1.05, and p-toluenesulfonic acid is used as a reaction catalyst. The mixture is heated to 160°C and reacted for 4 hours under a nitrogen stream. The reaction catalyst and unreacted oleic acid are then removed to obtain the final product.

[0031] Example 2

[0032] A crude oil direct-oiling spinning oil agent comprises the following components: 70 parts of a composite smoothing agent, 15 parts of an emulsifier, 4 parts of a penetrant, 6 parts of an antistatic agent, and 5 parts of a solvent. The composite smoothing agent comprises 25 parts of tetradecyl tetradecyl-9-enoate and 75 parts of PEG-12 dipalmitate. The emulsifier is sodium dioctyl sulfosuccinate, the penetrant is potassium perfluorooctyl sulfonate, the antistatic agent is an alkyl alcohol phosphate, and the solvent is water.

[0033] The following method was used to prepare the product: After adjusting the temperature inside the reactor to 45°C, tetradecyl tetradec-9-enoate and PEG-12 dispalmitate were added and stirred at 800 rad / min for 20 min. Then, alkyl alcohol phosphate was added and stirred for 15 min. After that, water and potassium perfluorooctyl sulfonate were added and stirred for 30 min. Finally, sodium dioctyl sulfonate was added as an emulsifier and stirred for 20 min. After cooling to room temperature, the product was filtered to obtain the final product.

[0034] Example 3

[0035] A crude oil direct-oiling spinning oil agent comprises the following components: 65 parts of a composite smoothing agent, 15 parts of an emulsifier, 4 parts of a penetrant, 6 parts of an antistatic agent, and 10 parts of a solvent. The composite smoothing agent comprises 30 parts of tetradecyltetradec-9-enoate and 70 parts of PEG-12 dipalmitate. The emulsifier is sodium dodecylbenzenesulfonate. The penetrant is composed of sodium perfluorooctanesulfonate and potassium perfluorooctanesulfonate in a mass ratio of 1:2. The antistatic agent is alkyl alcohol polyoxyethylene ether sulfonate, and the solvent is water.

[0036] The following method was used to prepare the product: After adjusting the temperature inside the reactor to 42°C, tetradecyltetradec-9-enoate and PEG-12 dispalmitate were added and stirred at 1200 rad / min for 20 min. Then, alkyl alcohol polyoxyethylene ether sulfonate was added and stirred for 20 min. After that, water, sodium perfluorooctyl sulfonate, and potassium perfluorooctyl sulfonate were added and stirred for 40 min. Finally, sodium dodecylbenzene sulfonate was added as an emulsifier and stirred for 60 min. After cooling to room temperature, the product was filtered to obtain the final product.

[0037] Comparative Example 1

[0038] The same technical solution as in Example 1 is adopted, except that the composite smoothing agent is composed of 20 parts of tetradecyl tetradec-9-enoate and 80 parts of PEG-12 dipalmitate.

[0039] Comparative Example 2

[0040] The same technical solution as in Example 1 is adopted, except that the composite smoothing agent is composed of 40 parts of tetradecyl tetradec-9-enoate and 60 parts of PEG-12 dipalmitate.

[0041] Comparative Example 3

[0042] The same technical solution as in Example 1 is adopted, except that the composite smoothing agent is composed of 35 parts of tetradecyl tetradec-9-enoate and 65 parts of mineral oil.

[0043] Comparative Example 4

[0044] The same technical solution as in Example 1 is adopted, except that the composite smoothing agent is composed of a mixture of white oil and fatty acid ester in a mass ratio of 1:1.

[0045] Comparative Example 5

[0046] The same technical solution as in Example 1 was used, except that the following method was used to prepare the mixture: the temperature inside the reactor was adjusted to 40°C, and tetradecyl tetradec-9-enoate, PEG-12 dispalmitate, alkyl alcohol phosphate polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and monooleate were mixed and stirred at 1000 rad / min for 60 min. After that, water was added and stirred for 20 min. After cooling to room temperature, the mixture was filtered to obtain the final product.

[0047] Comparative Example 6

[0048] TMT-217L, a spinning oil imported from Japan.

[0049] The spinning oils prepared in Examples 1-3 and Comparative Examples 1-5, as well as commercially available oils, were tested using the following methods: a) Transmittance: The particle uniformity and stability of the 15% emulsion were examined at 660 nm using a UV / Vis spectrometer; b) Volatilization loss: 1.0 ml of oil sample was dropped onto a steel test piece, baked in an oven at 230°C for 40 minutes, and characterized by the residual percentage; c) The spinning oil was placed in a sand bath and heated at 300°C for 3 hours, and then further heated in an electric furnace at 500°C for 5 hours. The heating residue rate was calculated by the weight change before and after heating, and the results are shown in Table 2.

[0050] Polyester polymer was melted and the spinning oils prepared in Examples 1-3 and Comparative Examples 1-5, as well as commercially available oils, were applied at a rate of 0.8% using a guided oiling method. The filaments were then stretched with hot rollers at 140°C to obtain 83d / 36f (fineness / filament number) polyethylene terephthalate FDY filaments. The uniformity and static friction coefficient of the produced filaments were tested, and the results are shown in Table 2. The uniformity of the filaments was characterized by the capacitance change of the filaments driven by a parallel plate capacitive sensor at a speed of 50 cm / min, using existing technology.

[0051] Table 2. Physicochemical properties of spinning oils and their impact on yarn production.

[0052]

[0053] As shown in Table 2, compared with Comparative Examples 1 and 2, the final light transmittance is higher and basically equivalent to that of Comparative Example 4 due to the specific proportion of composite smoothing agent in Examples 1-3 of this application. This indicates that the spinning oil prepared by the present invention has good emulsion stability. Compared with Example 1, Examples 2 and 3 select anionic surfactants containing fluorine as penetrants. The negatively charged sulfonate ions are adsorbed at the interface through electrostatic interaction, which can significantly reduce the surface tension of the final spinning oil. This can effectively prevent the accumulation of oil stains in the 500°C radiant heater and also enable the oil to form a more uniform lubricating film layer on the fiber surface, thereby significantly reducing the yarn breakage rate. In addition, the reduction of oil stains can significantly extend the cleaning cycle of the heater while ensuring that the heater has good heat conduction efficiency.

[0054] For Comparative Examples 3 and 4, when using conventional mineral oil, although the thermal stability and residue rate at 500℃ were comparable to those of Examples 1-3, the transmittance decreased significantly, indicating poor emulsion stability of the final spinning oil. Simultaneously, the uniformity of the prepared yarn decreased, while the static friction coefficient increased, indicating that the yarn quality was not ideal. For Comparative Example 5, although the only difference from Example 1 was the order of material addition in the preparation method, the physicochemical properties of the final spinning oil were significantly different, especially the transmittance. This indicates that changing the process order affects the emulsion stability of the final oil. In fact, even slight adjustments to the addition order can affect the final transmittance, which will not be elaborated further due to space limitations. The spinning oils prepared using Examples 1-3 of this application resulted in yarns with reduced friction coefficients and improved uniformity, even surpassing imported oils, thus improving yarn quality and performance.

[0055] While the present invention has been disclosed above, it is not limited thereto. Any person skilled in the art can make various modifications and alterations without departing from the spirit and scope of the invention; therefore, the scope of protection of the present invention should be determined by the scope defined in the claims.

Claims

1. A crude oil direct-oiling spinning oil agent, characterized in that, It includes 65-75% of a composite smoothing agent, which is composed of 25-35 parts of myristyl myristate and 65-75 parts of PEG-12 dipalmitate; The preparation method of the crude oil direct-oil type spinning oil agent includes the following steps: adjust the temperature in the reaction vessel to 38-45℃, add the composite smoothing agent according to the amount, stir at 800-1400 rad / min for 10-50 min, then add the antistatic agent and stir for 10-40 min, then add the solvent and penetrant and stir for 20-50 min, finally add the emulsifier and stir for 30-90 min, cool to room temperature and filter to obtain the product.

2. The crude oil direct-oiling spinning oil agent according to claim 1, characterized in that, The crude oil direct-oil spinning oil agent is composed of 65-75 parts of composite smoothing agent, 10-15 parts of emulsifier, 2-4 parts of penetrant, 2-6 parts of antistatic agent, and 6-10 parts of solvent, with water as the solvent. The composite smoothing agent is composed of 25-35 parts of myristyl myristate and 65-75 parts of PEG-12 dipalmitate.

3. The crude oil direct-oiling spinning oil agent according to claim 2, characterized in that, The emulsifier is selected from at least one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, cashew phenol polyoxyethylene ether, castor oil polyoxyethylene ether, sorbitan fatty acid ester, sorbitan polyoxyethylene ether fatty acid ester, or polyethylene glycol fatty acid ester.

4. The crude oil direct-oiling spinning oil agent according to claim 2, characterized in that, The penetrant is at least one of fatty alcohol polyoxyethylene ether, potassium perfluorooctane sulfonate, and sodium perfluorooctane sulfonate.

5. The crude oil direct-oiling spinning oil agent according to claim 2, characterized in that, The antistatic agent is selected from at least one of alkyl alcohol phosphate polyoxyethylene ether, alkyl alcohol phosphate, alkyl alcohol sulfonate, alkyl alcohol polyoxyethylene ether sulfonate, alkyl alcohol sulfate, alkyl alcohol ether sulfate salt, alkyl alcohol ammonium oxide, and betaine.

6. The crude oil direct-oiling spinning oil agent according to claim 1, characterized in that, The pH of the crude oil direct-oil spinning agent is 7.5-8.

0.

7. The crude oil direct-oiling spinning oil agent according to claim 1, characterized in that, The process includes the following steps: Adjust the temperature inside the reactor to 40-45℃, add the composite smoothing agent according to the specified amount, stir at 800-1200 rad / min for 10-30 min, then add the antistatic agent and stir for 10-20 min, then add the solvent and penetrant and stir for 20-40 min, finally add the emulsifier and stir for 30-60 min, cool to room temperature and filter to obtain the final product.

8. The application of a crude oil direct-oiling spinning oil agent as described in any one of claims 1-7 in the spinning production process.

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